Process of producing nitrogen-containing compounds



Feb. 12 1924.

J. H. REID PROCESS OF PRODUCING NITROGEN CONTAINING COMPOUNDS Filed Nov. 14, 1919 Patented i2, 322%,

JES E. REID, OF PITTSBURGH, PENNSYLVANIA, ASSIGNOR TO INTERNATIONAL NITROGEN (10., OF CLEVELAND, OHIO, A CORPORATION OF DELAWARE PROCESS F PRODUCING NITROGEN-CONTAINING COMPOUNDS.

Application filed Hovember 14, 1919. Serial Np. 338,109.

T 0 all whom it may concern:

Be it known that 1, JAMES H. Ran), a citizen of the United States, residing at Pittsbur h, in the county of Allegheny and State a of ennsylvania, have invented a certain new and useful Improvement in Processes of Producing llitrogen-Containing Compounds of which the following is a full, clear, an exact description, reference being had to the accompanying drawings. Y

This invention relates to a process for the manufacture of nitrogen-containing compounds and more particularly to the production of such compounds from carbide subjected to nitrogen in the resence of heat. It

is the general object of t e invention to produce such compounds in a particularly cilicient and economical manner.

Further and more limited objects of the invention will appear hereinafter and will be realized in and through the combinations of steps embodied in the claims annexed hereto. i

In the drawings formin part hereof, there is shown an apparatus w ereby the process may be realized in an effective manner. In said drawings, Fig. 1 represents a longitu dmal'sectional view through such apparatus; and Fig. 2 a sectional view corresponding to the line 2--2 of Fig. l and looking in the direction of the arrows.

Describing the parts by reference characters, vi denotes generally a furnace made of suitable fire-resistant material. For convenience of description, the left-hand. end 2 of the furnace shown in Fig. 1 is referred to as the front and the opposite end 3 as the rear. Above the top of the furnace there is shown a charging bell 4 such as is employed with acetylene, generators and blast furnaces. The bell is provided with a removable scaling cover 5 having an opening therethrough from which there extends a rod 6, forming an air-tight connection therewith, said rod carrying at its lower end a conical valve 7 cooperating with the lower frusto-conical end 8 of the hopper or bell. This valve stem or rod is shown as adjustable by being threaded into a collar 9- carried by spider arms 10 secured to the body t the bell or hopper. Extending downdicated at' 32*.

rear end of the furnace and communicating at its rear end with a similar chamber or retort 13, which in turn communicates at its front end with a similar chamber or retort 14. As many of these chambers may be cmployed as is desirable, depending upon the size of the furnace and the desired rate of production of the nitrified product. The rear end of the chamber 14 discharges through a vertical fine 15 into a closed receptacle 16, the flue being provided between said receptacle and the bottom wall of the furnace with a suitable valve 17 for sealing the said flue. The lower nd of the flue 15 projects considerably below the top of the receptacle 16, for a purpose to be described hereinafter.

Extending longitudinally of each of the chambers 12, 13 and 14 is a shaft, the said shafts being indicated at 18, 19 and 20, respectively. The shafts extend through the ends of their respective chambers and are .mounted in journals 21 provided on the front and rear walls of the furnace and are provided with driving means, such as pulleys 22 and 23, the shaft 19 having an additional pulle 24C- The shaft 20 is provided with a pul ey 25 shown as located at the front end thereof. The pulley 25 is adapted to receive power from any suitable power shaft (not shown) the power being transmitted through pulleys 25 and 28 and a belt 26 to the shaft 19 and by pulleys 22 and a belt 27 to shaft 18,

The chambers 12, 13 and 14; are circular in cross-section and each of the shafts is pro-;

vided within its chamberwith a screw feed conveyor, the said conveyors being indicated at 28, 29 and 30. Thefurnace 3 will be provided with any suitable means for heating the chambers 12, 13 and 14, a fluid burner 31 being indicated for this purpose.

Communicating with each of the reto'rts or chambers and preferably with the delivery end thereof, is a pipe indicated respectively at 32, each rovided with a valve inommunioating with each pipe 32 is a pipe 34 projecting thereinto. The pipes 32 serve to deliver nitrogen into each chamber or retort and the pipes serve to deliver into each of the nitrogen pipes an agent capable of activating the combination of the nitrogen with the carbide. For this purpose, a finely divided nitrate may beemployed. The nitrogen; be ing under a pressure of about 4 pounds per square inch, will serve to exhaust such activating agent. from the pipes 34 and to inject the same into the retorts or chambers.

In practising my process by an apparatus such as shown herein, I introduce into the charging bell t finely ground carbide. as calcium carbide. having first displaced the air from the retorts or chambers by circulat ing nitrogenthrough the same by means of the pipes 32 and the outlet pipe The carbide is fed through the retorts or chambers by means of the screw conveyors and is heated to about G50'C;'-in the atmosphere of nitrogen thereinxAt this stage the valves 32 and 35 will be opened and. adjusted so as to supply to each of the retorts or chambers nitrogen under a pressure of about 4 pounds to the square inch. The valves (not shown) in the pipes 34 being opened, the nitrogen Swill inject the activating agent into each retort and the carbides therein will be subjected tothe action of the nitrogen and the activatingagent suspended therein.

A great advantage in injecting the activating agent with the nitrogen resides in the saving of time required for the nitrification of the carbide and the efiiciency of the operation. As is well known, the combining of nitrogen with carbide is an exothermic reaction, the heat evolved being suflicient to raise the temperature of the mass about 75 C.

By blowing in the activating agent with the free nitrogen I obtain at once a rise in temperature of the mass in each retort and a quick combination of the nitrogen with the carbide by reason of the strong and virile condition of the activating agent, which is used while at its highest point of efficiency. Where an activating agent is mingled with the carbide and introduced therewith into the retorts, it will have become weakened to the extent to which it has combined with the carbide before coming under the in fluence of the free nitrogen and the nitrification proceeds much more slowly than where such agent is mingled with the nitrogen and introduced therewith.

Both the quickness and the completeness of the combination of nitrogen with the carbide are facilitated by subjecting the material to be nitrified to mixtures of nitrogen with the activating agent applied successively to the said material during its transit through the zone ofheat; also by the progressive heating of the material as it travels from the top of the retort assembly to the bottom of such assembly, where the source of heat is located.

Having thus described my invention, what I claim is 1. The process of producing a nitrified product which consists in conducting the material to be nitrified through a progressively heated zone and subjecting the carhide in such zone to an atmosphere of nitrogen having an activating agent mingled therewith.

2. The process of producing a nitrified product which consists in conducting the material to be nitrified through a progressively heated Zone containing a mixture of an activating agent with nitrogen under super-atmospheric pressure.

3. The process of producing a nitrified product which comprises feeding the material to be nitrified through a zone of heat and subjecting the heated carbide while in transit to the action of mixtures of nitrogen with an activating agent applied succes sively thereto.

4:. The process of producing a nitrified product which comprises feeding the mate rial to be nitrified through a; zone of heat and subjecting it while in transit to the action of mixture of nitrogen with activating agent applied successively thereto.

5. The process of producing a nitrified product which consists in continuously feeding an agitated mass of the material to be nitrified through a zone of heat and subjecting such heated mass to the action of successively applied mixtures of nitrogen, under super-atmospheric pressure, with an activating agent.

6. The process of producing a nitrified product which consists in conducting the material to be nitrified through a zone of heat, subjecting the heated material to the successive action of mixtures of nitrogen, under superatmospheric pressure. with an activating agent, and agitating the masswhile in transit through such zone.

7. The process of producing a nitrified product which consists in subjecting a heated mass ofmaterial to be nitrified to the action of a mixture of nitrogen and an RC? tivating agent supplied to the said material, and agitating the said material during the operation.

8. The process of producing a nitrified product which consists in conducting the material to be nitrified along a progressively heated retort and subjecting the said material to the action of a. mixture of nitrogen and an activating agent supplied there 12 to while in transit.

9. The process of producing a nitrifiedproduct which consists in conducting ana agitated mass of the material to be nitrified ture of nitrogen and an activating agent said retort, a mixture of nitrogen and an supplied to the retort adjacent to the de activating agent directed into .said retort l0 livery end thereof. ill-opposition to the movement of said mate- .10. The process of producing a nitrified rial therealong.

v 5 product which consists in conducting an In testimony whereof, I hereunto afiix my agitated mass of the material to be nitrified signature; i through a heated retort and supplying 0% said mass, adjacent to the delivery en JAMES H. REID. 

